Formation of Ag nanoparticles in transparent mica glass-ceramics

Formation of Ag nanoparticles in transparent mica glass-ceramicsSeiichi Taruta ⁎, Aya Mizoguchi, Tomohiko Yamakami, Tomohiro Yamaguchi Faculty of Engi...

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Journal of Non-Crystalline Solids 455 (2017) 52–58

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Formation of Ag nanoparticles in transparent mica glass-ceramics Seiichi Taruta ⁎, Aya Mizoguchi, Tomohiko Yamakami, Tomohiro Yamaguchi Faculty of Engineering, Shinshu University, 4-17-1, Wakasato, Nagano 380-8553, Japan

a r t i c l e

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Article history: Received 1 July 2016 Received in revised form 10 September 2016 Accepted 16 October 2016 Available online 24 October 2016 Keywords: Glass-ceramics Crystallization Mica Silver nanoparticles

a b s t r a c t Transparent or translucent mica glass-ceramics containing metallic Ag nanoparticles could be prepared by heating the 1–40 mol% Ag2O added parent glasses at 700–850 °C. A part of Ag+ ions added to the parent glasses as Ag2O was reduced to metallic Ag by the evolution of ﬂuorine from the parent glasses during heating above 700 °C, and then the specimens were colored in yellow or brown. At 700–800 °C, the size of metallic Ag particles was b 10 nm and became smaller slightly with an increase in additive amount of Ag2O. The shape was spherical while the rod-like Ag nanoparticles sandwiched between layers of micas were also observed in the specimens to which a smaller amount of Ag2O was added. The spherical Ag nanoparticles formed in mica structure at ≤800 °C grew preferentially to the parallel direction to the layer of micas at 850 °C together with the remarkable growth of micas to the parallel direction to the layer and then the shape varied to the rod-like. The rod-like Ag nanoparticles with width of 1–2 nm and length of b40 nm were sandwiched between layers of micas and oriented to the parallel direction to the layer. © 2016 Elsevier B.V. All rights reserved.

1. Introduction Recently, the reports on the glasses dispersed metallic Ag nanoparticles are increasing drastically [1]. The attractive optical properties of such glasses are generated by the surface plasmon resonance in metallic Ag nanoparticles, which is caused by interaction between the incoming electric ﬁeld and the free electrons conﬁned in the silver nanoparticles [1–4]. While the glasses colored by the surface plasmon resonance have been used as the glass artworks like the stained glass since literally millennia [1,5], the glasses containing noble metal nanoparticles such as Ag nanoparticles have a huge potential for technological applications in the optical and photonic devices [1–7]. The conventional preparation method of such glasses is ion-exchange followed by thermal treatment [2,8]. Other methods such as melt quenching [9,10], ion implantation [11,12], sol-gel techniques [13,14], or ion-exchange followed by ion or laser irradiation [15,16] and so on are also used to prepared such glasses. The details on the silver-doped glasses are recently reviewed by Gonella [1]. On the other hand, transparent glass-ceramics are interesting hosts for phosphors used for white LED, laser materials and so on. For example, transparent oxyﬂuoride glass-ceramics, based on ﬂuoride crystals dispersed throughout a continuous silicate glass, have been shown to combine the optical advantages of rare-earth-doped ﬂuoride crystals with the ease of forming and handling of conventional oxide glasses [17]. So very many studies on the luminescent properties of rare⁎ Corresponding author at: Department of Materials Chemistry, Faculty of Engineering, Shinshu University, 4-17-1 Wakasato, Nagano 380-8553, Japan. E-mail address: [email protected] (S. Taruta).

http://dx.doi.org/10.1016/j.jnoncrysol.2016.10.016 0022-3093/© 2016 Elsevier B.V. All rights reserved.

earth-doped transparent glass-ceramics are reported even in recent years [18–32]. Also, we succeeded in preparing novel machinable transparent glass-ceramics in which the ﬂuorine-micas were separated [33,34]. In addition, we could prepare Eu or Ce-doped transparent mica glass-ceramics [35,36]. The Eu-doped parent glasses emitted red light due to Eu3+ ions which were added as Eu2O3 while the mica glass-ceramics emitted purple light due to not only Eu3 + ions but also Eu2 + ions to which Eu3 + ions were reduced by heating the parent glasses in air [35]. In the same way, Ce4+ ions in the parent glasses were reduced to Ce3+ ions [36]. These reductions might be caused by the evolution of ﬂuorine from the glasses during heating in air. So we inferred that noble metallic ions such as Au+ and Ag+ ions which are doped to the parent glasses of the transparent mica glass-ceramics will be reduced to metal by heating the parent glasses to be crystallized. In this study, 1–40 mol% Ag2O was added to the starting materials of the transparent mica glass-ceramics. The parent glasses were prepared using such mixtures and then heated in air to be crystallized. So the reduction of Ag+ ions to metallic Ag and the inﬂuence of Ag2O addition on the crystallization of the parent glasses and the microstructure development of the obtained glass-ceramics were investigated. 2. Experimental procedure The composition of base glass in this study was corresponding to 70.4 mol% Li1·5Mg3AlSi4·5O13.25F2 + 29.6 mol% MgF2 (94.9 mass% Li1·5Mg3AlSi4·5O13.25F2 + 5.1 mass% MgF2). From this base glass, the transparent mica glass-ceramic could be prepared [34]. 0, 1, 5, 10, 15, 20, 25, 30, 35 and 40 mol% Ag2O were added to the raw materials of

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850°C

800°C

750°C

700°C

650°C

Parent glasses

(a)

(b)

(c)

(d)

(e)

Fig. 1. Photographs of parent glasses and the heated parent glasses at 650 °C, 700 °C, 750 °C, 800 °C and 850 °C for 1 h. (a) Ag-1, (b) Ag-10, (c) Ag-20, (d) Ag-30 and (e) Ag-40 specimens.

: mica : silver

: mica : silver

: Chondrodite : β-Eucryptite

: β-Eucryptite

(e)

(f)

Intensity / a.u.

(e)

(d)

Intensity / a.u.

(d) (c) (b)

(c) (b)

(a)

(a) 20

40 2θ / °CuKα

60

Fig. 2. XRD patterns of (a) Ag-20 parent glass and Ag-20 specimen heated at (b) 650 °C, (c) 700 °C, (d) 750 °C, (e) 800 °C and (f) 850 °C for 1 h.

20

40 2θ / °CuKα

60

Fig. 3. XRD patterns of (a) Ag-1, (b) Ag-10, (c) Ag-20, (d) Ag-30 and (e) Ag-40 specimens heated at 800 °C for 1 h.

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Basal spacing (c·sinβ β) / Ǻ

10.1 10

(DTA). The microstructures of the glass-ceramics were observed using a transmission electron microscope (TEM) and a scanning transmission electron microscope (STEM).

Trisilicic type mica

3. Results

9.9

Tetrasilicic type mica

3.1. Crystallization

9.8 9.7

Ag-20 Ag-25 Ag-35 Ag-30 Ag-15 Ag-40 Ag-10 Ag-5

9.6 9.5

Ag-1

Ag-0

9.4 9

9.05

9.1

9.15

9.2

Lattice constant (b) / Ǻ Fig. 4. Relationship between basal spacing (c·sinβ) and lattice constant (b) of micas separated in (○) Ag-0 and (●) Ag-1 to − 40 specimens heated at 750 °C for 1 h. Trisilicic type mica: (◇ [36], ◆ [37]) K-phlogopite (KMg3(AlSi3O10)F2). Tetrasilicic type mica: (△ [38], ▲ [39]) K-taeniolite (KMg2Li(Si4O10)F2), (□ [38]) Na-taeniolite (NaMg2Li(Si4O10)F2), and (■ [40]) K-tetrasilisic mica (KMg2.5(Si4O10)F2).

the base glass and mixed. For example, the meaning of 40 mol% Ag2O addition to the raw materials is corresponding to the composition of 60 mol% base glass + 40 mol% Ag2O. The mixtures were melted in a sealed platinum container at 1200–1450 °C for 2 h, and then cooled outside of the furnace. The obtained glasses were annealed at about 20 °C higher temperatures (550–570 °C) than their glass-transition temperatures for 1 h and then cooled at 2 °C/min to eliminate strain. The parent glasses prepared by such a method were cut to dimensions of about 5 mm × 5 mm × 1 mm and were heated at 600–850 °C for 1 h in air to be crystalized. Such specimens were shown as Ag-0, Ag-1, Ag-5, Ag10, Ag-15, Ag-20, Ag-25, Ag-30, Ag-35 and Ag-40, respectively, according to the additive amount of Ag2O, in this paper. The thermally change of the parent glasses was analyzed using an Xray diffraction (XRD) analyzer and a differential thermal analyzer

(a)

Photographs of the parent glasses and the heated parent glasses are shown in Fig.1. Every parent glass was transparent and colorless. Crystals were not detected in almost parent glasses by XRD analysis while a very small amount of mica appeared in the XRD patterns of the Ag-1 and Ag-10 parent glasses. All of the specimens were colored in yellow or brown by heating at ≥ 700 °C. The specimens to which a larger amount of Ag2O was added were colored more uniformly over the whole specimens and tended to be colored in brown. Such coloring should be contributed to the surface plasmon resonance in metallic Ag nanoparticles formed by heating the parent glasses. That is, these photographs suggest that Ag nanoparticles were formed in all specimens heated at ≥ 700 °C. Furthermore, the specimens to which a larger amount of Ag2O, especially 40 mol% Ag2O, was added maintained transparency or translucency even at higher temperatures although they were colored in darker. XRD patterns of the Ag-20 parent glass and the heated Ag-20 specimens are shown in Fig. 2. Mica appeared at 650 °C and trace of chondrodite (Mg5(SiO4)2F2) which acts as nuclei for mica was observed. Crystalline phase detected at 700 °C was only mica and then a large amount of β-eucryptite separated at 750 °C. (This β-eucryptite was βeucryptite solid solution [33].) Metallic Ag was not detected at ≤ 750 °C although the specimens were colored in brown (Fig.1(c)). DTA results show that the crystallization temperatures of chondrodite, mica and β-eucryptite tended to be lowered slightly by the addition of Ag2O, which were not shown in this paper as DTA curves, however, the crystallization process of the parent glasses containing Ag2O was almost the same with that of the parent glass to which Ag2O was not added. Metallic Ag was detected at ≥800 °C. In the XRD patterns of the specimens to which N 15 mol% Ag2O were added, metallic Ag was observed above 800 °C. XRD patterns of the specimens heated at 800 °C are shown in Fig. 3. The diffraction peaks of metallic Ag were observed for the Ag-20, Ag-30

(b)

20nm

(c)

20nm

(d)

20nm

20nm

Fig. 5. STEM images of (a) Ag-5 and (c) Ag-10 specimens heated at 700 °C, and Z-contract images of (b) Ag-5 and (d) Ag-10 specimens heated at 700 °C.

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(a)

20nm (b)

500nm (c)

55

(060), respectively. The obtained basal spacing and lattice constant b are shown in Fig. 4. In addition, the reported basal spacing and lattice constant b of trisilicic type mica [37,38] and tetrasilicic type micas [39–41] are plotted as references in Fig. 4. In general, the basal spacing, which is the distance between basal planes in the vertical direction to the layer, depends mainly on the size of the interlayer cations and the electrostatic repulsion between layers. The lattice constant b is a standard for determining whether the mica is the tetrasilicic or trisilicic type and the b of tetrasilicic type micas is shown to be smaller than that of trisilicic type micas. The composition of mica separated in the Ag-0 specimen was Li(Mg2 + yLi1 − y)(AlySi4 − y)O10F2 (0 b y b 1) [34]. The chemical formula means that the interlayer cations were Li+ ions, the octahedral sheets contained Li+ and Mg2+ ions and the tetrahedral sheets contained Al3+ and Si4+ ions. So Fig. 4 indicates that the mica separated in the Ag-0 specimen had the smaller basal spacing than other micas having larger interlayer ions such as Na+ and K+ ions. And compared with the basal spacing of mica in the Ag-0 specimen, that of micas in the specimens to which N 5 mol% Ag2O were added became larger. However, the lattice constant b was not almost varied by the addition of Ag2O. That is, Li+ ions in the layers of micas in these specimens were substituted by Ag+ ions having larger size than other cations in the specimens because the structure of the micas becomes more stable. So if all of Li+ ions in layers of micas are substituted by Ag+ ions, the basal spacing will be the intermediate value between that of K-type micas (K-phlogopite and K-taeniolite) and that of Na-type micas (Na-taeniolite) because the ionic radius (1.29 Å) of Ag+ ion is the intermediate value between that (1.52 Å) of K+ ion and that (1.16 Å) of Na+ ion. In actual fact, their basal spacing was almost the same with that of Na-taeniolite or smaller, which means that a part of Li+ ions in the layers was substituted by Ag+ ions. The basal spacing of the micas tended to become larger with an increase in the additive amount of Ag2O up to 20 mol%, and smaller with further addition. In this way, a part of Ag+ ions, which was not reduced, remained in the layers of micas. However, even if an additive amount of Ag2O is increased, Ag+ ions in the layers of micas will not be always increased. 3.2. Microstructure

1μ μm Fig. 6. STEM images of Ag-40 specimen heated at (a) 700 °C, (b) 800 °C and (c) 850 °C.

and Ag-40 specimens, but their intensities were almost the same in spite of the additive amount of Ag2O and heating temperatures (800 °C and 850 °C). These results suggest that a part of Ag+ ions was reduced to metallic Ag by heating the specimens and the others remained as Ag+ ions in the specimens. On the other side, a large amount of mica separated in all specimens. As other crystal phases, βeucryptite appeared in all specimens heated at ≥750 °C, however, the diffraction peak intensity of β-eucryptite was weaker with an increase in additive amount of Ag2O. The separation of β-eucryptite made the obtained mica glass-ceramics opaque [33,34]. However, the mica glass-ceramics to which a larger amount of Ag2O was added maintained transparency or translucency even when β-eucryptite separated. The basal spacing (c·sinβ; c and β are lattice constants) and lattice constant b of micas separated in the specimens heated at 750 °C were determined from the diffraction peaks of lattice plane (003) and

STEM and Z-contrast images of the Ag-5 and Ag-10 specimens heated at 700 °C are shown in Fig. 5. The Z-contrast is proportional to square of the atomic number. That is, the Z-contrast images of these specimens show the difference in Ag concentration and the lighter places in the images contain a larger amount of Ag. The STEM and Z-contrast images in Fig. 5 (a) and (b) are the same place in the specimen, but the Z-contrast image are a little shifted to upper right direction. In the STEM image (Fig. 5 (a)), the micas having layered structure were observed. The size of the long axis direction which is parallel direction to the layer was b 100 nm and that of the short axis direction which is vertical direction to the layer was b 30 nm. And the dark spherical particles with size of b 10 nm and dark rod-like particles sandwiched between layers of micas were observed. In the Z-contrast image (Fig. 5 (b)), these dark particles appeared as well lighted-images. That is, such particles are metallic Ag nanoparticles. Similarly, micas having layered structure and spherical metallic Ag nanoparticles with size of b 10 nm were observed in the Fig. 5 (c) and (d) although the rod-like Ag nanoparticles were not. These metallic Ag nanoparticles in all specimens heated at 700 °C were not detected by XRD analysis, but STEM and Z-contrast images conﬁrmed their existence. STEM images of the Ag-40 specimen heated at 700–850 °C are shown in Fig. 6. At 700 °C, micas having layered structure were observed. The sizes of the long axis direction of micas in the Ag-5, Ag-10 and Ag-40 specimens heated at 700 °C were valued from the Fig. 5 (a), (c) and Fig. 6 (a), and they were b 100 nm, b 30 nm and b20 nm, respectively. This indicates that the size of the micas in the specimens tended to be smaller with an increase in the additive amount of Ag2O. The metallic Ag nanoparticles which were observed as the dark

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(a)

(b)

20nm

20nm Fig. 7. TEM images of Ag-40 specimen heated at (a) 800 °C and (b) 850 °C.

spherical particles were several nanometers. At 800 °C, micas grew to the size of b500 nm and the spherical large particles with size of b400 nm, which should be β-eucryptite, were also observed, nevertheless, the specimen was transparent. At 850 °C, the micas grew much more, and the size of the long axis direction was several micrometers. The β-eucryptite grew slightly. Nevertheless, the specimen showed translucency. In Fig. 6 (b) and (c), the metallic Ag particles were not clear, then high magniﬁcation TEM and STEM images of the Ag-40

specimen heated at 800 and 850 °C are shown in Fig. 7 and Fig. 8, respectively. At 800 °C, spherical Ag nanoparticles with size of b 10 nm were formed in mica structure (Fig. 7 (a)), and at 850 °C, rod-like Ag nanoparticles were sandwiched between the layers of micas (Fig. 7 (b) and Fig. 8 (a)). The size of the long axis direction of larger rod-like Ag nanoparticles was 40 nm and that of the short axis direction of the rod-like Ag nanoparticles was 1–2 nm. The width of the rod-like Ag nanoparticles was about one time to two times of the basal spacing of micas.

(b)

(a)

50nm

20nm

(c)

(d)

β-eucriptite

mica

50nm

50nm

(f)

(e)

β-eucriptite

200nm

200nm

Fig. 8. STEM images of Ag-40 specimen heated at (a, b) 850 °C and (c, e) 800 °C and Z-contract images of (e, f) Ag-40 specimen heated at 800 °C.

TG curve

0 1 2 3

Weight Loss / %

S. Taruta et al. / Journal of Non-Crystalline Solids 455 (2017) 52–58

Intensity/ a.u.

Mass number: 19 (F2) Mass number 2 (H2) 18 (H2O) 20 (HF) 32 (O2) 85 (SiF4)

200

400

600

800

1000

1200

Heating Temperature / °C Fig. 9. TG and mass spectra curves of Ag-10 parent glass.

4. Discussion 4.1. Separation of metallic Ag nanoparticles Our previous studies [35,36] suggest that the reduction of rare earth ions, such as Eu3+ and Ce4+ ions, might be caused by the evolution of ﬂuorine from the glasses during heating in air. Also, in the reduction of Ag+ ions to metallic Ag, ﬂuorine evaporated from the specimens seems to play an important role. Then, the gas phases evaporated from the specimens during heating in the ﬂow of He gas were analyzed using a mass spectrometer with thermogravimetric (TG) analyzer. The TG curve and changes in intensities of mass spectra of the Ag-10 parent glass during heating are shown in Fig. 9. The TG curve shows that when the heating temperature is raised, the weight loss began about at 700 °C and 2 wt% of specimen was lose at 1200 °C. The mass spectra show that F2 (mass number: 19) gas was evaporated from the Ag-10 parent glass at ≥700 °C, and other gases were not. So the weight loss of the specimen resulted from the evolution of F2 from the specimen. That is, F− ions in the specimens were evaporated by heating at ≥700 °C, and Ag+ ions in the specimens were reduced to metallic Ag in order to maintain the electrical neutrality of the specimens. It is concluded that the reduction of Ag+ ions in the specimens to metallic Ag was caused by the evolution of F2 from specimens. 4.2. Growth of metallic Ag nanoparticles In the TEM and STEM images of the Ag-40 specimens heated at 800 and 850 °C (Fig. 7, Fig. 8 (b), (c) and (e)), dark stripes appeared along the parallel direction to the layer of micas. So in the Z-contrast images which are the same place in the specimens (Fig. 8 (d) and (f)), dark stripes in the STEM images appeared as well lighted stripes. Some stripes in Fig. 8 (e) and (f) are shown by arrows. That is, in the stripes, Ag might be concentrated. Besides, compared STEM images in Fig. 8 (c) and (e) with Z-contrast images in Fig. 8 (d) and (f), it is clear that Ag+ ions or metallic Ag nanoparticles contained in β-eucryptite were much less (Fig. 8 (d) and (f)). These results suggest that Ag+ ions were concentrated in a part of the layers of micas but not in the βeucryptite. In the mica structure in which Ag+ ions were concentrated, the spherical Ag nanoparticles with size of b10 nm were formed at ≤ 800 °C (Fig. 7 (a)), and then they grew preferentially to the parallel

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direction to the layer of micas at 850 °C together with the remarkable growth of micas to the parallel direction to the layer (Fig. 7 (b) and Fig. 8 (a)). That is, Ag nanoparticles were enlarged to the parallel direction to the layer by the growth of micas. As the results, the size of Ag nanoparticles became much larger along the parallel direction to the layer and became smaller in the vertical direction to the layer. So the shape of Ag nanoparticles was varied to the rod-like, and the rod-like Ag nanoparticles were sandwiched between layers of micas and oriented to the parallel direction to the layer. In the Ag-5 specimen heated at 700 °C, the rod-like Ag nanoparticles were observed. In the Ag-5 specimen, micas grew larger to the size of b100 nm even at 700 °C. Therefore, small spherical Ag nanoparticles formed at ≤700 °C grew to the parallel direction to the layer of largely grown micas at 700 °C. Consequently, Ag nanoparticles became rod-like shape even at 700 °C. Such spherical and rod-like Ag nanoparticles generated the surface plasmon resonance and the specimens were colored in yellow or brown. 5. Conclusions In this study, 1–40 mol% Ag2O was added to the starting materials of the transparent mica glass-ceramics having composition of 70.4 mol% Li1·5Mg3AlSi4·5O13.25F2 + 29.6 mol% MgF2. The parent glasses were prepared using such mixtures and then heated in air to be crystallized. At 700 °C, the mica separated in all specimens. For the micas separated in the specimen to which 5 mol% Ag2O was added, the size of the parallel direction to the layer was b 100 nm and that of the vertical direction to the layer was b30 nm. These sizes tended to become smaller with an increase in the additive amount of Ag2O. Also, at 700 °C, the specimens were colored in yellow or brown by the surface plasmon resonance in metallic Ag nanoparticles. Although the metallic Ag was not detected by XRD analysis, the existence was conﬁrmed by STEM and TEM observation. The Ag nanoparticles in the specimens heated at ≥ 800 °C were detected by XRD analysis. β-eucryptite separated at 750 °C and the micas grew to several micrometers at 850 °C. The specimens lost the transparency at higher temperatures, however, the specimen to which 40 mol% Ag2O was added maintained translucency even at 850 °C. A part of Ag+ ions added to the parent glasses was reduced to metallic Ag above 700 °C by the evolution of ﬂuorine from the specimens. At 700 °C, the shape of the Ag nanoparticles was spherical while the rod-like Ag nanoparticles sandwiched between layers of micas were also observed in the specimens to which a smaller amount of Ag2O was added. The size of spherical Ag particles was b 10 nm and became smaller slightly with an increase in additive amount of Ag2O. The spherical Ag nanoparticles formed in mica structure at ≤ 800 °C grew preferentially to the parallel direction to the layer of micas at 850 °C together with the remarkable growth of micas to the parallel direction to the layer and the shape varied to the rod-like. As the results, the rod-like Ag nanoparticles with width of 1–2 nm and length of b40 nm were sandwiched between layers of micas and oriented to the parallel direction to the layer. References [1] F. Gonella, Silver doping of glasses, Ceram. Int. 41 (2015) 6693–6701. [2] A. Ajami, W. Husinsky, B. Svecova, S. Vytykacova, P. Nekvindova, Saturable absorption of silver nanoparticles in glass for femtosecond laser pulses at 400 nm, J. Non-Cryst. Solids 426 (2015) 159–163. [3] A.V. Redkov, V.V. Zhurikhina, A.A. Lipovskii, Formation and self-arrangement of silver nanoparticles in glass via annealing in hydrogen: the model, J. Non-Cryst. Solids 376 (2013) 152–157. [4] L. Li, Y. Yang, D. Zhou, X. Xu, J. Qiu, The inﬂuence of Ag species on spectroscopic features of Tb3+-activated sodium–aluminosilicate glasses via Ag+–Na+ ion exchange, J. Non-Cryst. Solids 385 (2014) 95–99. [5] A. Simo, J. Polte, N. Pfänder, U. Vainio, F. Emmerling, K. Rademann, Formation mechanism of silver nanoparticles stabilized in glassy matrics, J. Am. Chem. Soc. 134 (2012) 18824–18833. [6] A. Quaranta, E. Cattaruzza, F. Gonella, A. Rahman, G. Mariotto, Cross-sectional Raman micro-spectroscopy study of silver nanoparticles in soda–lime glasses, J. Non-Cryst. Solids 401 (2014) 219–223.

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